反应详情

To a solution of 1 ml. of diethylamine in 5 ml. of dry dimethylformamide, 350 mg. of 8-bromo-1-(chloromethyl)-6-(2-pyridyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine (obtained as in Preparation 3) is added and the mixture stirred under nitrogen at room temperature for about 4.5 hours. To the mixture, 50 mg. of sodium iodide is added and stirring is continued at room temperature for about 18 hours and then heated at about 100 to about 110° C. for about an additional 6 hours. It is then poured into ice water and extracted with chloroform. The extract is washed with water, dried over anhydrous potasssium carbonate and concentrated under vacuum. The residue is crystallized from ethyl acetate: Skellysolve B to give pure 8-bromo-1-[(diethylamino)methyl]-6-(2-pyridyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine (I).

1. stirringstirring
2. waitis continued at room temperature for about 18 hours
3. temperatureheated at about 100 to about 110° C. for about an additional 6 hours
4. extractionextracted with chloroform
5. washThe extract is washed with water
6. dry with materialdried over anhydrous potasssium carbonate
7. concentrationconcentrated under vacuum
8. customThe residue is crystallized from ethyl acetate